Mass spectrometry (MS) will be utilized to develop methods for quantitative analysis and structure determination which are applicable to minimum quantity (10 to the minus 6th power - less than 10 to the minus 12th power g) samples of importance to biomedical and health-oriented problems. General areas of research include: (1) Improved Instrumental Techniques: continuous monitoring of high-pressure liquid chromotographs (LC/MS): structure determination of complex molecules utilizing collisional activation (CA) spectra to determine fragment structures corresponding to individual MS peaks; and the analysis of complex mixtures from biological samples through mass spectral separation followed by CA identification of the separated molecular ion species. (2) Automation of Analytical Methods: improvements to the high-resolution (HR) MS/computer (COM) system to incorporate Signal Enhancement in Real-Time, and improvements to the CA-MS/COM system for automatic acquisition and identification of CA peaks in normal mass spectra and in spectra of mixture molecular ions. (3) Mass Spectrometry Theory: classification of mass spectral reactions, unimolecular ion decomposition mechanisms, ion structures, and activated complex geometries and other parameters of the Quasi-Equilibrium Theory.